CN106521175A - Method for recycling sliver from precipitates generated in test - Google Patents
Method for recycling sliver from precipitates generated in test Download PDFInfo
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- CN106521175A CN106521175A CN201610936272.1A CN201610936272A CN106521175A CN 106521175 A CN106521175 A CN 106521175A CN 201610936272 A CN201610936272 A CN 201610936272A CN 106521175 A CN106521175 A CN 106521175A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
- C22B11/042—Recovery of noble metals from waste materials
- C22B11/044—Recovery of noble metals from waste materials from pyrometallurgical residues, e.g. from ashes, dross, flue dust, mud, skim, slag, sludge
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- Chemical & Material Sciences (AREA)
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- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for recycling silver from precipitates generated in a test. The method comprises the following steps of: testing precipitates of gold, sliver, palladium, platinum and rhodium as raw materials through a fire assay method, wherein silver chloride and other less impurities are main components, water mass accounts for about 65%, and silver chloride mass accounts for about 35%; drying the precipitates, anhydrous sodium carbonate and anhydrous borax in a mass ratio being 1 to (1-2) to (0.5-1), and uniformly mixing to obtain a mixture; putting the mixture into a heat-resistant container, covering a layer of anhydrous sodium sulfate on the heat-resistant container, heating the mixture to 1100-1300 DEG C within 30-50 minutes and preserving the heat for 10-30 minutes; after cooling the mixture, adding a hydrochloric acid solution with concentration being 5%, heating and boiling, and washing with water, thereby obtaining recycled sliver. The invention provides the method for recycling sliver through the fire method, and the method is simple to operate, realizes high efficiency, low cost and no pollution in a recycling process, and is suitable for recycling silver in precipitates generated in fire-assaying test.
Description
Technical field
The present invention relates to a kind of recovery method of silver, the method that silver is reclaimed in more particularly to a kind of sediment from test.
Background technology
Detection precious metal element is typically enriched with using Fire Assaying, needs to add a certain amount of fine silver in Fire Assaying enrichment process
Protective agent and enrichment trapping agent are blown as noble metal ash, while the silver in argentiferous sample is also enriched with, fine silver addition is at least big
Three times of noble metal total amount in sample are general to add 40 milligrams or so of fine silver every time.In test process, silver first passes through nitric acid
Dissolving is converted into silver nitrate solution, and Jing chloroazotic acid is processed silver nitrate solution again, and the precious metal element such as gold, palladium, platinum is converted into chloride
Exist in solution, silver nitrate then occurs precipitation reaction with chlorion and is converted into silver nitride precipitation, is deposited on test container bottom.
The sediment is most of to be present with silver chlorate form, wherein being mingled with a small amount of other impurity.This can all be produced using Fire Assaying test
Sediment is planted, a small amount of sediment is produced every time, is not collected during cleaning container in the past and just outwell, all of sediment is received
Collection gets up, and takes care of the pence.In sediment, up to tens milligrams, silver belongs to precious metal element to silver content, and in reclaiming sediment, silver has
Important economic worth, had both avoided the wasting of resources, and environmental protection, significant to developing a circular economy.At present, reclaim
The method of silver has wet method, pyrogenic process, wet method and pyrogenic process to be used in combination.Wet method is first by strong acid, highly basic leaching silver, then passes through reduction
Or electrolytic method reclaims silver；Pyrogenic process is smelted under high temperature by adding appropriate flux, and separation and concentration reclaims silver.Pyrogenic process is reclaimed
Rate is low, and the purity for reclaiming silver is low.Wet bench is complicated, and impurity separating difficulty is big.For different material selects different silver recovery
Method.For the method that silver is reclaimed from the test sediment produced by Fire Assaying enrichment yet there are no pertinent literature report.
The content of the invention
It is an object of the invention to reclaim silver from test sediment, there is provided a kind of method that pyrogenic process reclaims silver, realize back
Receipts process rapidly and efficiently, it is inexpensive, pollution-free.The method is using Fire Assaying test gold, silver, palladium, platinum, the collected sediment of rhodium
For raw material, its main component is silver chlorate, wherein it is mingled with other a small amount of impurity, such as：Copper, lead, bismuth, tin, silicate etc., wherein water
Sub-prime amount accounts for 65%, and silver chlorate quality accounts for 35%.Before reclaiming silver, sediment heat drying is smashed after cooling again.
Technical scheme is as follows：Dry sediment in mass ratio:Natrium carbonicum calcinatum:Borax anhydrous=1:1~2:0.5
~ 1, after being well mixed, it is placed in heatproof container, covers one layer of anhydrous sodium sulfate above, it is warmed up to 1100 in 30 ~ 50 minutes ~
1300 DEG C, 10 ~ 30min is incubated, after cooling, adds 5% hydrochloric acid solution, heating to boil, then wash with water, be recycled
Silver.
Sodium carbonate in the present invention plays smelting flux and antichlor effect, and borax anhydrous landing low melting point and slag making are made
With.Natrium carbonicum calcinatum is used alone or borax anhydrous recovering effect is undesirable, be used in mixed way natrium carbonicum calcinatum and borax anhydrous is returned
The surface of cash register is clean, smooth.Natrium carbonicum calcinatum and borax anhydrous addition are few, and the rate of recovery is low, and amount can not be significantly improved back greatly
Yield, also wastes flux, heats up too fast, and smelting temperature is too low, temperature retention time is too short, and recovering effect is bad；Smelting time is long,
Temperature is too high, has both wasted the energy, also proposes requirements at the higher level to equipment, and recovering effect is poor.By optimizing drying sediment and flux
Proportioning, control pyrometallurgical smelting temperature and smelting time reclaims silver from the sediment produced by Fire Assaying testing experiment.We
Method is simple to operate, cost recovery is low, pollution-free, it is adaptable to reclaim the silver in the sediment produced by Fire Assaying test.
Specific embodiment
The present invention is further elaborated with reference to embodiment.With collected by Fire Assaying test gold, silver, palladium, rhodium etc.
Sediment is raw material, the moisture ＜ 65% of sediment, moisture ＜ 2% after being dried.
Embodiment 1：Fire Assaying tests sediment composition analysis result such as table 1 below：
The Fire Assaying test sediment composition of 1 the present embodiment of table
| Element | Ag | Cl | Ca | Fe | Mg | Si | H2O |
| Content/% | 75.1 | 24.7 | 0.03 | 0.02 | 0.02 | 0.12 | ＜ 0.5 |
50 grams of 100 grams of dry sediments, 100 grams of natrium carbonicum calcinatum and borax anhydrous are weighed, is put in heatproof container, is stirred
Afterwards, one layer of anhydrous sodium sulfate is covered above, be placed in high temperature furnace, 1300 DEG C are warmed up in 50 minutes, be incubated 30min, cooling
After take out, remove surface residual debris be put in container, the hydrochloric acid solution for plus 5%, heating boil, remove with water clean, be recycled silver
73.0 grams, purity is more than 99.9%, the rate of recovery 97.2%.
Embodiment 2：Fire Assaying tests sediment composition analysis result such as table 2 below：
The Fire Assaying test sediment composition of 2 the present embodiment of table
| Element | Ag | Cl | Ca | Fe | Mg | Si | H2O |
| Content/% | 73.9 | 24.4 | 0.02 | 0.02 | 0.03 | 0.15 | ＜ 2 |
50 grams of 50 grams of dry sediments, 100 grams of natrium carbonicum calcinatum and borax anhydrous are weighed, is put in heatproof container, is stirred
Afterwards, one layer of anhydrous sodium sulfate is covered above, be placed in high temperature furnace, 1100 DEG C are warmed up in 30 minutes, be incubated 10min, cooling
After take out, remove surface residual debris, be put in container, the hydrochloric acid solution for plus 5%, heating boil, remove with water clean, be recycled
36.5 grams of silver, purity are more than 99.9%, the rate of recovery 98.8%.
Claims (1)
1. a kind of method that silver is reclaimed in sediment from test, tests the sediment of gold, silver, palladium, platinum, rhodium as original with fire assaying
Material, main component is silver chlorate and other a small amount of impurity, and biodiversity accounts for 65%, and silver chlorate quality accounts for 35%, it is characterized in that
Dry sediment in mass ratio:Natrium carbonicum calcinatum:Borax anhydrous=1:1~2:0.5 ~ 1, after being well mixed, it is placed in heatproof container,
One layer of anhydrous sodium sulfate is covered above, 1100 ~ 1300 DEG C are warmed up in 30 ~ 50 minutes, be incubated 10 ~ 30min, after cooling, plus
Enter 5% hydrochloric acid solution, heating is boiled, and then washes with water, the silver being recycled.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610936272.1A CN106521175B (en) | 2016-11-01 | 2016-11-01 | A method of recycling silver from test sediment |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610936272.1A CN106521175B (en) | 2016-11-01 | 2016-11-01 | A method of recycling silver from test sediment |
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| Publication Number | Publication Date |
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| CN106521175A true CN106521175A (en) | 2017-03-22 |
| CN106521175B CN106521175B (en) | 2018-09-04 |
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| CN201610936272.1A Active CN106521175B (en) | 2016-11-01 | 2016-11-01 | A method of recycling silver from test sediment |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR910005056B1 (en) * | 1988-08-19 | 1991-07-22 | 방세훈 | Method for refining of au. ag |
| CN1186866A (en) * | 1997-11-27 | 1998-07-08 | 夏新民 | Wet silver extracting process from silver ore with high manganese, sulphur and iron content |
| CN102373338A (en) * | 2010-08-20 | 2012-03-14 | 沈阳有色金属研究院 | Method for extracting metallic silver from silver chloride sediment |
| CN103451435A (en) * | 2013-09-02 | 2013-12-18 | 浙江触捷光电科技有限公司 | Method for recovering metal silver from waste in silver pulp screen printing process |
-
2016
- 2016-11-01 CN CN201610936272.1A patent/CN106521175B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR910005056B1 (en) * | 1988-08-19 | 1991-07-22 | 방세훈 | Method for refining of au. ag |
| CN1186866A (en) * | 1997-11-27 | 1998-07-08 | 夏新民 | Wet silver extracting process from silver ore with high manganese, sulphur and iron content |
| CN102373338A (en) * | 2010-08-20 | 2012-03-14 | 沈阳有色金属研究院 | Method for extracting metallic silver from silver chloride sediment |
| CN103451435A (en) * | 2013-09-02 | 2013-12-18 | 浙江触捷光电科技有限公司 | Method for recovering metal silver from waste in silver pulp screen printing process |
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| CN106521175B (en) | 2018-09-04 |
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Address after: 510000 363 Changxin Road, Tianhe District, Guangzhou, Guangdong. Patentee after: Industrial analysis and testing center of Guangdong Academy of Sciences Address before: 510651 No. 363, Changxin Road, Guangzhou, Guangdong, Tianhe District Patentee before: GUANGDONG INDUSTRY ANALYSIS TESTING CENTER |
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